反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of 1-(3-aminopropyl)-4-[2-pyridyl]pyridinium bromide hydrobromide (6 g, 16 mmol) in MeOH (150 mL) at 0-5° C. was added NaBH4 (2 g, 53 mmol) in small portions over a period of 2 h. The reaction mixture was stirred overnight at room temperature and the solvent was evaporated. The residue was suspended in ether (200 mL) and treated with 50% NaOH solution (100 mL). The ether layer was separated and the aqueous layer was extracted with more ether (2×50 mL). The combined ether extracts were dried over potassium carbonate and the solvent was removed to give 3-(3′,6′-dihydro-2′-H-[2,4′]bipyridinyl-1′-yl)-propylamine (3.48 g) as an oil. It was used in the next step immediately without purification.
WORKUP
后处理
- customthe solvent was evaporated
- additiontreated with 50% NaOH solution (100 mL)
- customThe ether layer was separated
- extractionthe aqueous layer was extracted with more ether (2×50 mL)
- dry with materialThe combined ether extracts were dried over potassium carbonate
- customthe solvent was removed